CN103387328B - The production method of the rose-colored rear-earth-doped silica tube of a kind of low hydroxyl - Google Patents
The production method of the rose-colored rear-earth-doped silica tube of a kind of low hydroxyl Download PDFInfo
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- CN103387328B CN103387328B CN201210154059.7A CN201210154059A CN103387328B CN 103387328 B CN103387328 B CN 103387328B CN 201210154059 A CN201210154059 A CN 201210154059A CN 103387328 B CN103387328 B CN 103387328B
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Abstract
The invention discloses the production method of the rose-colored rear-earth-doped silica tube of a kind of low hydroxyl, belong to silica tube manufacturing technology field, comprise the following steps: (1) material choice: choose high purity quartz; (2) stir: add in the feed samaric nitrate, etc. multiple rare earth nitrating agent carry out mix and blend; (3) dilute: add strong hydrofluoric acid and carry out diluting reaction; (4) adulterate: adulterate with high purity quartz powder, put into high temperature resistant silica tube; (5) dry: carry out high temperature continuous drying, make various nitrating agent penetrating in quartz powder materials completely; (6) melting: drop in continuous induction melting furnace and carry out melting, through tube drawing bench traction, produces the rose-colored silica tube of integral colouring; (7) deshydroxy: rose-colored silica tube is put into vacuum deshydroxy stove and carry out high temperature deshydroxy.Be mainly used in silica tube manufacture view.
Description
Technical field
The present invention relates to silica tube manufacturing technology field, particularly relate to the production method of the rose-colored rear-earth-doped silica tube of a kind of low hydroxyl.
Background technology
Technology contents closest to red silica tube: utilize the red silica tube that high purity quartz raw material doped with rare-earth elements oxide compound is produced, rare earth element and the ratio of its doping are cupric nitrate 0.1 ~ 5%, europium sesquioxide 0.1 ~ 5%, magnesium oxide 0.1 ~ 5%, after mixing oven dry with high purity quartz raw material, can the red silica tube of direct production through to drop in continuous induction melting furnace, but coloring effect is bad, caliber scope and wall thickness deflection are comparatively large, and also easily fade, color uniformity is inconsistent.
Technology contents closest to blue silica tube: utilize the blue silica tube that high purity quartz raw material doped with rare-earth elements oxide compound is produced, its doping rare earth element and ratio be three phosphatization alum account for raw material 0.1 ~ 5%, titanium oxide 0.1 ~ 5%, cobalt oxide 0.1 ~ 5%, after mixing oven dry with high purity quartz raw material, can the blue silica tube of direct production through to drop in continuous induction melting furnace, but coloring effect is bad, caliber scope and wall thickness deflection are comparatively large, and also easily fade, color uniformity is inconsistent.
Summary of the invention
In order to overcome above-mentioned defect, the present invention proposes the production method of the rose-colored rear-earth-doped silica tube of a kind of low hydroxyl, the technical scheme of employing is as follows:
A production method for the rose-colored rear-earth-doped silica tube of low hydroxyl, concrete steps are as follows:
(1) material choice: choose high purity quartz, wherein SiO2 >=99.99999%, as the doped raw material of rose-colored silica tube doped with rare-earth elements nitrating agent;
(2) stir: by weight be the samaric nitrate of raw material 0.1 ~ 15%, 0.1 ~ 15% aluminum nitrate, the saltpetre of 0.1 ~ 15%, zinc nitrate, the nitrate of baryta of 0.1 ~ 15%, the multiple nitrating agent of SODIUMNITRATE of 0.1 ~ 15% of 0.1 ~ 15%, adopt and be not more than the warm water of 80 DEG C, the total amount of water is not more than 60 kilograms of multiple nitrating agent weight and carries out mix and blend with raw material;
(3) dilute: add the strong hydrofluoric acid being not more than various nitrating agent total amount 15% and carry out diluting and adding fast response, enable various nitrating agent Homogeneous phase mixing;
(4) adulterate: adulterate with high purity quartz powder 80-160 order, after stirrer uniform stirring, it is put into high temperature resistant silica tube;
(5) dry: carry out high temperature 200 DEG C of-250 DEG C of continuous dryings, in drying course, the quantity according to required drying material suitably adjusts temperature, and various nitrating agent is penetrated into completely in high purity quartz powder in hyperthermia drying process;
(6) melting: after abundant cooling, then to drop in continuous induction melting furnace 1800 DEG C-2200 DEG C and carry out melting, through tube drawing bench traction, direct production can go out the rose-colored silica tube of integral colouring;
(7) deshydroxy: rose-colored silica tube is put into vacuum deshydroxy stove and carry out high temperature deshydroxy, hydroxyl, within the scope of 800 DEG C ~ 1050 DEG C, 3 ~ 8 hours deshydroxy time, is reduced to 1 ~ 30ppm by temperature.。
Preferably: the high temperature resistant quartzy pipe range 2.6m of step (4), diameter 200mm, wall thickness 6mm.
Preferably: the suitable setting range of the temperature of step (5) is 210 DEG C-250 DEG C.
Preferably: step (7) deshydroxy temperature is 950 DEG C-1000 DEG C, the deshydroxy time is 5 hours.
The advantage of the production method of the rose-colored rear-earth-doped silica tube of a kind of low hydroxyl of the present invention is as follows:
More red and blue silica tube is compared, what adulterate is not rare earth oxide, the present invention is doped with different solid element nitrating agents, and increase the per-cent of raw material weight, simultaneously, after uniform stirring and hyperthermia drying, reach uniformly penetrating and get rid of moisture content, when dropping into continuous induction melting furnace melting, fusing thoroughly and the material property keeping quartz raw material intrinsic and purity do not changed, adulterate in high purity quartz raw material multiple rare earth nitrating agent, and the rose-colored silica tube of direct production, form good coloring effect, rose-colored silica tube integral colouring, caliber scope and wall thickness deflection less, simultaneously, after high temperature deshydroxy, rose-colored silica tube is colour-fast, color uniformity is consistent, hydroxyl can within the scope of 1 ~ 30ppm, belong to the rose-colored doped silica glass pipe of the low hydroxyl of high-quality, technique effect is obvious, the rose-colored silica tube of external coating (EC) can be substituted completely.
Embodiment
A production method for the rose-colored rear-earth-doped silica tube of low hydroxyl, concrete steps are as follows:
(1) material choice: choose high purity quartz, wherein SiO
2>=99.99999%, as the doped raw material of rose-colored silica tube doped with rare-earth elements nitrating agent;
(2) stir: by weight be the samaric nitrate of raw material 0.1 ~ 15%, 0.1 ~ 15% aluminum nitrate, the saltpetre of 0.1 ~ 15%, zinc nitrate, the nitrate of baryta of 0.1 ~ 15%, the multiple nitrating agent of SODIUMNITRATE of 0.1 ~ 15% of 0.1 ~ 15%, adopt and be not more than the warm water of 80 DEG C, the total amount of water is not more than 60 kilograms of multiple nitrating agent weight and carries out mix and blend with raw material;
(3) dilute: add the strong hydrofluoric acid being not more than various nitrating agent total amount 15% and carry out diluting and adding fast response, enable various nitrating agent Homogeneous phase mixing;
(4) adulterate: adulterate with high purity quartz powder 80-160 order, after stirrer uniform stirring, it is put into high temperature resistant silica tube;
(5) dry: carry out high temperature 200 DEG C of-250 DEG C of continuous dryings, in drying course, the quantity according to required drying material suitably adjusts temperature, and various nitrating agent is penetrated into completely in high purity quartz powder in hyperthermia drying process;
(6) melting: after abundant cooling, then to drop in continuous induction melting furnace 1800 DEG C-2200 DEG C and carry out melting, through tube drawing bench traction, direct production can go out the rose-colored silica tube of integral colouring;
(7) deshydroxy: rose-colored silica tube is put into vacuum deshydroxy stove and carry out high temperature deshydroxy, hydroxyl, within the scope of 800 DEG C ~ 1050 DEG C, 3 ~ 8 hours deshydroxy time, is reduced to 1 ~ 30ppm by temperature.
The above; be only the specific embodiment of the present invention, but the protection domain of invention is not limited thereto, any those of ordinary skill in the art are in the technical scope that the present invention discloses; the change that can expect easily or replacement, within the protection domain that all should be encompassed in invention.
Claims (5)
1. a production method for the rose-colored rear-earth-doped silica tube of low hydroxyl, concrete steps are as follows:
(1) material choice: choose high purity quartz, wherein SiO
2>=99.99999%, as the doped raw material of rose-colored silica tube doped with rare-earth elements nitrating agent;
(2) stir: by weight be the samaric nitrate of raw material 0.1 ~ 15%, 0.1 ~ 15% aluminum nitrate, the saltpetre of 0.1 ~ 15%, zinc nitrate, the nitrate of baryta of 0.1 ~ 15%, the multiple nitrating agent of SODIUMNITRATE of 0.1 ~ 15% of 0.1 ~ 15%, adopt and be not more than the warm water of 80 DEG C, the total amount of water is not more than 60 kilograms of multiple nitrating agent weight and carries out mix and blend with raw material;
(3) dilute: add the strong hydrofluoric acid being not more than various nitrating agent total amount 15% and carry out diluting and adding fast response, enable various nitrating agent Homogeneous phase mixing;
(4) adulterate: adulterate with high purity quartz powder 80-160 order, after stirrer uniform stirring, it is put into high temperature resistant silica tube;
(5) dry: carry out high temperature 200 DEG C of-250 DEG C of continuous dryings, in drying course, the quantity according to required drying material suitably adjusts temperature, and various nitrating agent is penetrated into completely in high purity quartz powder in hyperthermia drying process;
(6) melting: after abundant cooling, then to drop in continuous induction melting furnace 1800 DEG C-2200 DEG C and carry out melting, through tube drawing bench traction, direct production can go out the rose-colored silica tube of integral colouring;
(7) deshydroxy: rose-colored silica tube is put into vacuum deshydroxy stove and carry out high temperature deshydroxy, hydroxyl, within the scope of 800 DEG C ~ 1050 DEG C, 3 ~ 8 hours deshydroxy time, is reduced to 1 ~ 30ppm by temperature.
2. the production method of the rose-colored rear-earth-doped silica tube of a kind of low hydroxyl according to claim 1, is characterized in that: the high temperature resistant quartzy pipe range 2.6m of described step (4), diameter 200mm, wall thickness 6mm.
3. the production method of the rose-colored rear-earth-doped silica tube of a kind of low hydroxyl according to claim 1, is characterized in that: the suitable setting range of the temperature of described step (5) is 210 DEG C-250 DEG C.
4. the production method of the rose-colored rear-earth-doped silica tube of a kind of low hydroxyl according to claim 1, is characterized in that: described step (7) deshydroxy temperature is 950 DEG C-1000 DEG C.
5. the production method of the rose-colored rear-earth-doped silica tube of a kind of low hydroxyl according to claim 1, is characterized in that: the deshydroxy time of described step (7) is 5 hours.
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Families Citing this family (5)
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| CN103641300B (en) * | 2013-11-26 | 2016-01-13 | 连云港市盛昌照明电器有限公司 | High purity quartz preparation method and for cryogenic heat exchanger silica tube and preparation method |
| CN103641302A (en) * | 2013-12-02 | 2014-03-19 | 连云港福东正佑照明电器有限公司 | Low-hydroxyl low-melting-point transparent quartz tube and preparation method thereof |
| CN105837010A (en) * | 2016-04-21 | 2016-08-10 | 太仓市建兴石英玻璃厂 | Preparation method of high-performance quartz tube |
| CN106242277A (en) * | 2016-08-04 | 2016-12-21 | 江苏圣达石英制品有限公司 | A kind of rear-earth-doped water process quartz ampoule and preparation method thereof |
| CN106746637A (en) * | 2017-02-20 | 2017-05-31 | 单祥发 | A kind of production method of low oxyhydroxide and rear-earth-doped quartz ampoule |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04300218A (en) * | 1991-03-28 | 1992-10-23 | Kokusai Denshin Denwa Co Ltd <Kdd> | Production of quartz glass doped with rare-earth element |
| CN1850679A (en) * | 2006-05-25 | 2006-10-25 | 单军成 | Method for producing low-hydroxy-group squartz glass tube |
| CN1850680A (en) * | 2006-05-25 | 2006-10-25 | 单军成 | Method for producing low-hydroxyl-group quartz glass tube |
| JP2007230814A (en) * | 2006-02-28 | 2007-09-13 | Shinetsu Quartz Prod Co Ltd | Method of manufacturing rare earth metal element-containing silica glass for optics |
| CN101717193A (en) * | 2009-12-10 | 2010-06-02 | 徐传龙 | Red infrared-penetrating quartz tube and preparation method thereof |
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2012
- 2012-05-10 CN CN201210154059.7A patent/CN103387328B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04300218A (en) * | 1991-03-28 | 1992-10-23 | Kokusai Denshin Denwa Co Ltd <Kdd> | Production of quartz glass doped with rare-earth element |
| JP2007230814A (en) * | 2006-02-28 | 2007-09-13 | Shinetsu Quartz Prod Co Ltd | Method of manufacturing rare earth metal element-containing silica glass for optics |
| CN1850679A (en) * | 2006-05-25 | 2006-10-25 | 单军成 | Method for producing low-hydroxy-group squartz glass tube |
| CN1850680A (en) * | 2006-05-25 | 2006-10-25 | 单军成 | Method for producing low-hydroxyl-group quartz glass tube |
| CN101717193A (en) * | 2009-12-10 | 2010-06-02 | 徐传龙 | Red infrared-penetrating quartz tube and preparation method thereof |
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Effective date of registration: 20170119 Address after: Cattle town Donghai County 222300 Jiangsu province Lianyungang Limin Road No. 27 Patentee after: Dan Xiangfa Address before: Fuhua road 222000 East Economic Development Zone Jiangsu city Lianyungang province No. 303 Patentee before: Lianyungang Dongxin Quartz Co., Ltd. |
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Effective date of registration: 20190417 Address after: 222300 Ruip Quartz Products Co., Ltd. in Guanzhuang Village, Niushan Town, Donghai County, Lianyungang City, Jiangsu Province Patentee after: Lianyungang Longli Quartz Products Co., Ltd. Address before: 222300 No. 27 Limin East Road, Niushan Town, Donghai County, Lianyungang City, Jiangsu Province Patentee before: Dan Xiangfa |